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Preparation method and application of palladium/bamboo charcoal catalyst

A catalyst and bamboo charcoal technology, which is applied in the field of palladium/bamboo charcoal catalyst preparation, can solve the problems of low crystallite content and low metal Pd dispersion

Active Publication Date: 2015-09-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In view of the low dispersion of metal Pd in ​​the catalyst that exists in the prior art, the problem that microcrystalline content is low, the invention provides a kind of preparation method of Pd / bamboo charcoal catalyst, the Pd / bamboo charcoal catalyst prepared by the inventive method is used for crude Hydrofining of isophthalic acid

Method used

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  • Preparation method and application of palladium/bamboo charcoal catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Take 500g commercially available bamboo charcoal material, the specific surface area is 550m 2 / g, the pore volume is 0.9mL / g, and the average pore (diameter) diameter is 6.5nm. The bamboo charcoal was acid-washed twice with 1.5 mol / L sulfuric acid at 75 °C, each treatment time was 2 h, the liquid-solid volume ratio was 3:1, and then washed until neutral and then dried. Prepare NO with sodium nitrite and water 2 The concentration is 0.05mol / L impregnation solution, equal volume impregnation active carbon carrier 8 hours, the preparation palladium weight content is 100 milliliters of the chloropalladium acid solution of 0.5%, then adjust the pH value to between 4~6 with alkali, stable 10 After ~200 minutes, the palladium-containing compound is supported by a spray-dipping method to obtain a catalyst precursor. After the catalyst precursor was aged for 12 hours, 20 grams of 5% sodium formate by weight and 200 grams of pure water were used to prepare a reducing solution,...

Embodiment 2

[0019] Bamboo charcoal was washed with 3 mol / L nitric acid at a washing temperature of 75°C, then washed with water until neutral, and the rest were the same as in Example 1. The catalyst product A-2 was obtained.

Embodiment 3

[0021] Bamboo charcoal is washed with the phosphoric acid of 5mol / L, and washing temperature is 80 ℃, then washes with water to neutrality, and all the other are with embodiment 1. The catalyst product A-3 was obtained.

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Abstract

The invention relates to a preparation method and application of a palladium / bamboo charcoal catalyst. The palladium / bamboo charcoal catalyst is used for selective hydrogenation of crude m-phthalic acid and mainly overcomes the problems of poor dispersion of metal Pd and low minicrystal content in and poor thermal stability of a catalyst in the prior art. According to the invention, bamboo charcoal is used as a carrier, a Pd-containing solution is used for dipping of or is sprinkled on pretreated bamboo charcoal to prepare the palladium / bamboo charcoal catalyst, palladium is uniformly dispersed on the surface and secondary surface of bamboo charcoal, and a reducing agent is used for reduction so as to obtain the palladium / bamboo charcoal catalyst with high activity. Compared with a traditional palladium / charcoal catalyst, the palladium / bamboo charcoal catalyst provided by the invention has better activity, a longer service life and higher mechanical compressive strength.

Description

technical field [0001] The invention relates to a preparation method and application of a palladium / bamboo charcoal catalyst, which is used for selective hydrogenation of crude isophthalic acid. Background technique [0002] Supported palladium / carbon catalysts are mainly used for the selective hydrogenation of unsaturated organic compounds. The crude isophthalic acid obtained by the oxidation of m-xylene contains a certain amount of by-product impurities, and the existence of m-carboxybenzaldehyde (3-CBA for short) affects the quality and color of polyester, and it is difficult to use the usual crystallization method remove. However, after the selective hydrogenation of the supported palladium / carbon catalyst into m-toluic acid, it can be separated and purified by crystallization. Since the palladium / carbon catalyst usually uses a single active component, the research on its improvement has been focused on the structure of the support and the distribution of metal Pd on t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44C07C63/24C07C51/487
Inventor 汤涛王少军凌凤香王敏
Owner CHINA PETROLEUM & CHEM CORP
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